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2-Methoxyethylamine → HCID 58459091、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Methoxyethylamine | HCID 8018 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 4,6-Dichloro-2-methylpyrimidin-5-amine | HCID 736674 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 58459091 | HCID 58459091 | 115.4% |
反応手順
Heat a solution of 4,6-dichloro-2-methyl-pyrimidin-5-ylamine (5.0 g, 0.02 mol), 2-methoxyethylamine (2.32 g, 0.03 mol) and diisopropylethylamine (3.9 g, 0.03 mol) in isopropanol (70 mL) at 150° C. in a sealed tube for 16 h. Cool the reaction mixture to room temperature, and remove the isopropanol under reduced pressure to give a residue. Dissolve the residue in dichloromethane and wash with water and brine. Dry the organic layer over anhydrous sodium sulfate, filter, and concentrate under reduced pressure to give a residue. Purify the residue on a silica gel column eluting with methanol:dichloromethane (4:96) to give the title compound (5.0 g). ES/MS m/z 217 (M+1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08759360B2 |
| 出典データセット | uspto-grants-2014_06 |
| ORD ID | ord-e1eff8e04c884e67bcddbb118d418b4e |
| 出典メモ | uspto-grants-2014_06 |